Pd/C催化对异丁基苯乙酮加氢生成对异丁基苯乙醇

Pd/C catalyzes the hydrogenation of IBAP to IBPE

目的通过试验制得高收率的对异丁基苯乙醇(IBPE),为下一步羰基合成布洛芬提供较纯的反应物。方法以异丁苯为起始原料经傅克酰基化自制的对异丁基苯乙酮(IBAP)通过加氢反应制得,并通过单因素试验法和正交试验法进行对异丁基苯乙醇(IBPE)合成工艺的研究。结果 30 g对异丁基苯乙酮,对异丁基苯乙酮∶甲醇(质量比)=1∶3,T=30℃,P=0.8 MPa,5%Pd/C 2.4 g,氢氧化钠(30%)0.38 g,反应时间3.2 h,在此工艺条件下对异丁基苯乙醇的收率可以达到96.5%。结论当活性金属Pd负载量较低以及反应条件相对温和的情况下更加有利于对异丁基苯乙醇收率的提高。

Objective A high yield ofp-isobutylphenylethanol(IBPE) was prepared experimentally to provide a relatively pure reactant for the next oxo synthesis of ibuprofen. Methods Isobutylbenzene was used as the starting material to prepare IBPE by hydrogenation reaction,and the synthesis process of IBPE was carried out by single factor experiment and orthogonal experiment. Results 30 g IBAP,m(IBAP):m(methanol)=1:3;T=30 ℃;P = 0.8 MPa;m (5% Pd/C)=2.4 g;m[NaOH (30%)]=0.38 g.The reaction time was 3.2 h,and the yield of IBPE can reach 96.5% under the process conditions. Conclusion The improvement of IBPE yield was more favorable when the active metal Pd loading was lower and the reaction conditions were relatively mild.